CN120992995A - Apparatus and methods for processing three-dimensional atomic probe samples - Google Patents
Apparatus and methods for processing three-dimensional atomic probe samplesInfo
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- CN120992995A CN120992995A CN202511025711.9A CN202511025711A CN120992995A CN 120992995 A CN120992995 A CN 120992995A CN 202511025711 A CN202511025711 A CN 202511025711A CN 120992995 A CN120992995 A CN 120992995A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/20—Sample handling devices or methods
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Abstract
本公开涉及材料分析的技术领域，例如涉及一种用于三维原子探针样品的处理装置和处理方法，处理装置包括：样品承载模组，设置有样品工位，每个样品工位用于安放一个三维原子探针样品；真空密封管，用于容纳样品承载模组；冷却模块，设置有用于容纳冷却液的腔室，腔室设置有密封管工位，密封管工位用于放置真空密封管。基于以上处理装置可以为三维原子探针样品的处理过程提供全流程的真空和低温保护机制，有助于显著提升后续材料相变分析和成分表征的准确性，确保了三维原子探针数据能够真实反映三维原子探针样品的微观结构特征。
This disclosure relates to the technical field of materials analysis, specifically to a processing apparatus and method for three-dimensional atomic probe samples. The processing apparatus includes: a sample carrier module with sample stations, each station for holding one three-dimensional atomic probe sample; a vacuum sealing tube for housing the sample carrier module; and a cooling module with a chamber for containing coolant, the chamber having a sealing tube station for holding the vacuum sealing tube. Based on this processing apparatus, a full-process vacuum and cryogenic protection mechanism can be provided for the processing of three-dimensional atomic probe samples, significantly improving the accuracy of subsequent material phase transition analysis and compositional characterization, and ensuring that the three-dimensional atomic probe data can truly reflect the microstructural characteristics of the three-dimensional atomic probe sample.
Description
Technical Field
The present disclosure relates to the technical field of material analysis, for example, to a processing apparatus and a processing method for a three-dimensional atom probe sample.
Background
Three-dimensional atom probe (Three-Dimensional Atom Probe,3 DAP) is a high-resolution material characterization technology capable of realizing atomic scale element distribution analysis. The basic principle is that a high-voltage pulse electric field is applied to a needle-tip-shaped three-dimensional atom probe sample, surface atoms of the three-dimensional atom probe sample are evaporated layer by layer in an ultrahigh vacuum environment, and the atomic species and the spatial position information thereof are detected by a time-of-flight mass spectrometer, so that a three-dimensional atomic-level structure inside the material is reconstructed. The technology is widely applied to component analysis and microstructure research in the fields of metal materials, semiconductor devices, nano structures and the like.
In the preparation process of a three-dimensional atom probe sample, a material to be measured is generally required to be roughly polished into a needle-shaped structure, and fine polishing is performed to obtain the end of the three-dimensional atom probe sample with nanometer size. However, certain environmentally sensitive alloy materials (e.g., age-hardened aluminum alloys, titanium alloys, nickel-based superalloys, etc.) exhibit room temperature parking effects during conventional sample preparation procedures. Specifically, after the three-dimensional atom probe sample is subjected to heat treatment, the three-dimensional atom probe sample is required to be exposed to a room temperature environment for transfer and secondary sample preparation (such as electrolytic polishing), and the process is difficult to avoid heat exchange between the material and the environment, so that a room temperature parking effect occurs, and the three-dimensional atom probe sample is caused to undergo phenomena such as component segregation, phase change or local precipitation, so that finally obtained three-dimensional atom probe data cannot accurately reflect the microstructure characteristics of the material, and the accurate characterization of the microstructure of the material under extreme process conditions is severely restricted.
In order to mitigate or suppress the parking effect, the residence time of the sample at room temperature, i.e. the time from the start of sample preparation to the introduction into the analysis chamber, needs to be minimized or avoided. During processing/transferring of three-dimensional atom probe samples, the related art may cause the sample to come into contact with air, thereby initiating oxidation. For example, in the process of performing heat treatment on the three-dimensional atom probe sample after rough polishing and transferring the three-dimensional atom probe sample to the fine polishing device, the sample is contacted with air to cause oxidization, and the rough polishing needs to be performed again, so that the time of a sample preparation process is increased. Although the related art provides a vacuum heat treatment apparatus or a low temperature transfer device for three-dimensional atom probe samples to improve pollution control and thermal stability during sample preparation, there is still a lack of vacuum environmental control for the whole process from heat treatment to low temperature transfer, and problems caused by oxidation of products and room temperature parking effect cannot be effectively overcome.
Disclosure of Invention
The following presents a simplified summary in order to provide a basic understanding of some aspects of the disclosed embodiments. This summary is not an extensive overview, and is intended to neither identify key/critical elements nor delineate the scope of such embodiments, but is intended as a prelude to the more detailed description that follows.
The embodiment of the disclosure provides a processing device and a processing method for a three-dimensional atom probe sample, provides a vacuum and low-temperature protection mechanism of a whole process, and remarkably improves the accuracy of phase change analysis and component characterization of subsequent materials.
According to a first aspect of the present disclosure there is provided a processing apparatus for a three-dimensional atom probe sample comprising:
the sample bearing module is provided with sample stations, and each sample station is used for placing a three-dimensional atom probe sample;
the vacuum sealing tube is used for accommodating the sample bearing module;
The cooling module is provided with a chamber for containing cooling liquid, and the chamber is provided with a sealing tube station used for placing a vacuum sealing tube.
In some embodiments, the sample carrier module comprises:
the sample bearing base is provided with a sample station;
The sample protection cover is detachably covered on the sample bearing base to place the sample station inside.
In some embodiments, the sample protection cover is provided with a through hole.
In some embodiments, the sample bearing base is a columnar structure with threads on the outer peripheral surface, and one end surface of the sample bearing base is provided with a sample station;
The sample protection cover is of a cylindrical structure with threads on the inner peripheral surface, and is covered and buckled on the sample bearing base in a threaded connection mode.
In some embodiments, one end face of the sample carrying base is provided with a plurality of sample stations.
In some embodiments, the sample protective cover comprises:
a bottom plate;
The inner peripheral surface of the cylinder is provided with threads, the bottom plate is arranged at one end of the cylinder, and the other end of the cylinder is open;
At least one of the bottom plate and the cylinder is provided with a through hole.
In some embodiments, the bottom plate is provided with a plurality of through holes.
In some embodiments, the cylinder is provided with a plurality of through holes distributed along the circumferential and/or axial direction of the cylinder.
In some embodiments, the cooling module comprises:
A housing provided with a chamber for accommodating a cooling liquid and having an opening;
the cover body is detachably arranged at the opening of the shell;
the sealing tube bearing seat is positioned in the cavity and is provided with a sealing tube station.
In some embodiments, the outer wall of the housing is a vacuum sandwich, and/or the outer wall of the housing is provided with a thermally insulating material.
In some embodiments, the seal tube carrier is provided with a plurality of seal tube stations.
In some embodiments, the seal tube carrier is a cylindrical structure, one end face of the seal tube carrier is connected to the bottom of the shell, and the other end face of the seal tube carrier is provided with a plurality of seal tube stations.
According to a second aspect of the present disclosure, there is provided a processing method for a three-dimensional atom probe sample, implemented based on the processing apparatus for a three-dimensional atom probe sample provided in the first aspect, comprising:
placing the coarsely polished three-dimensional atom probe sample at a sample station of a sample bearing module;
Placing the sample bearing module in a vacuum sealing tube, vacuumizing the vacuum sealing tube, and then performing heat treatment on the three-dimensional atom probe sample;
Placing the vacuum sealing tube after heat treatment at a sealing tube station of a cooling module, and cooling the three-dimensional atom probe sample by using cooling liquid;
and after cooling is completed, taking out the three-dimensional atom probe sample from the sample bearing module.
In some embodiments, the parameter requirements of the thermal treatment process of the three-dimensional atom probe sample include at least one of:
The temperature of the heat treatment is not lower than 300 ℃;
The duration of the heat treatment is not less than 10min;
the vacuum degree in the vacuum sealing tube is not higher than 1×10 -2 Pa.
In some embodiments, the parametric requirements of the desuperheating cooling process of the three-dimensional atom probe sample include at least one of:
the cooling rate is not lower than 10 ℃ per second;
the temperature of the three-dimensional atom probe sample after cooling is not higher than-50 ℃.
The processing device and the processing method for the three-dimensional atom probe sample provided by the embodiment of the disclosure can realize the following technical effects:
The processing device for the three-dimensional atom probe sample provided by the embodiment of the disclosure provides a whole-course vacuum protection environment for the three-dimensional atom probe sample through the vacuum sealing tube in the processing process applied to the three-dimensional atom probe sample. Specifically, the atomic probe sample was placed in a vacuum sealed tube after rough polishing to avoid contact with air. Then, the three-dimensional atom probe sample enters a heat treatment process, and accurate temperature control is realized through an external heating system. After the heat treatment is finished, the three-dimensional atom probe sample and the vacuum sealing tube are transferred to a cooling module together, and the cooling liquid is utilized for rapid cooling. Since the three-dimensional atom probe sample remains in a vacuum environment throughout the cooling process, contact with air is further prevented. In the heat treatment and cooling stage, the three-dimensional atom probe sample is always in a vacuum sealing state, so that the contact with the outside air is effectively isolated, and the three-dimensional atom probe sample is prevented from undergoing oxidation reaction, thereby being beneficial to shortening the preparation flow time of the three-dimensional atom probe sample. In the cooling stage, the cooling liquid in the cooling module can be used for rapidly cooling and keeping the low temperature for a long time, so that the problem of component segregation or phase change caused by the room temperature standing effect is avoided. Finally, after cooling, the three-dimensional atom probe sample is taken out from the vacuum sealed tube and subjected to finish polishing treatment, and then is rapidly transferred into three-dimensional atom probe equipment for characterization. Through the vacuum and low-temperature protection mechanism of the whole flow, the accuracy of phase change analysis and component characterization of the subsequent materials is obviously improved, and the three-dimensional atomic probe data can truly reflect the microstructure characteristics of the three-dimensional atomic probe sample.
The foregoing general description and the following description are exemplary and explanatory only and are not intended to limit the present disclosure.
Drawings
One or more embodiments are illustrated by way of example and not limitation in the figures of the accompanying drawings, in which like references indicate similar elements, and in which like reference numerals refer to similar elements, and in which:
FIG. 1 is a schematic diagram of a processing apparatus for three-dimensional atom probe samples at one perspective provided by embodiments of the present disclosure;
FIG. 2 is a schematic diagram of a processing apparatus for three-dimensional atom probe samples at one perspective provided by embodiments of the present disclosure;
FIG. 3 is a schematic diagram of a processing apparatus for a three-dimensional atom probe sample provided in an embodiment of the present disclosure, taken at A in FIG. 2;
FIG. 4 is a schematic illustration of a processing apparatus for three-dimensional atom probe samples provided in an embodiment of the present disclosure with a cover removed;
FIG. 5 is a schematic view of a vacuum seal tube provided by an embodiment of the present disclosure;
FIG. 6 is a schematic diagram of a sample carrier module provided in an embodiment of the present disclosure;
FIG. 7 is an exploded view of a sample carrier module according to an embodiment of the present disclosure;
fig. 8 is a flow diagram of a method for processing a three-dimensional atom probe sample according to an embodiment of the present disclosure.
The description of the reference numerals is as follows:
100 a processing device for a three-dimensional atom probe sample;
1, a sample bearing module;
a 101 sample station, a 11 sample bearing base and a 12 sample protection cover;
120 through holes, 121 bottom plates and 122 cylinder bodies;
2, vacuum sealing the tube;
3, a cooling module;
301 chamber, 302 seal tube station;
31 cover body, 32 shell body and 33 sealing tube bearing seat;
200 three-dimensional atom probe samples.
Detailed Description
So that the manner in which the features and techniques of the disclosed embodiments can be understood in more detail, a more particular description of the embodiments of the disclosure, briefly summarized below, may be had by reference to the appended drawings, which are not intended to be limiting of the embodiments of the disclosure. In the following description of the technology, for purposes of explanation, numerous details are set forth in order to provide a thorough understanding of the disclosed embodiments. However, one or more embodiments may still be practiced without these details. In other instances, well-known structures and devices may be shown simplified in order to simplify the drawing.
The terms first, second and the like in the description and in the claims of the embodiments of the disclosure and in the above-described figures are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate in order to describe embodiments of the present disclosure. Furthermore, the terms "comprise" and "have," as well as any variations thereof, are intended to cover a non-exclusive inclusion.
The term "plurality" means two or more, unless otherwise indicated.
In the embodiment of the present disclosure, the character "/" indicates that the front and rear objects are an or relationship. For example, A/B represents A or B.
The term "and/or" is an associative relationship that describes an object, meaning that there may be three relationships. For example, A and/or B, represent A or B, or three relationships of A and B.
The term "corresponding" may refer to an association or binding relationship, and the correspondence between a and B refers to an association or binding relationship between a and B.
Referring to fig. 1 to 7, the embodiment of the present disclosure provides a processing apparatus 100 for a three-dimensional atom probe sample, the processing apparatus 100 including a sample carrying module 1, a vacuum sealing tube 2, and a cooling module 3.
The sample carrier module 1 is provided with sample stations 101, each sample station 101 being for receiving one three-dimensional atom probe sample 200. The vacuum sealing tube 2 is used for accommodating the sample carrying module 1. The cooling module 3 is provided with a chamber 301 for containing a cooling liquid, the chamber 301 being provided with a sealing tube station 302, the sealing tube station 302 being for placing the vacuum sealing tube 2.
The processing device 100 can perform processing work before analysis on the three-dimensional atom probe sample 200. Specifically, the coarsely polished three-dimensional atom probe sample 200 is first placed in the sample station 101 of the sample carrier module 1. Each sample station 101 is adapted to a fixed copper tube of the three-dimensional atom probe sample 200, ensuring that the three-dimensional atom probe sample 200 remains stable during subsequent processing.
After the three-dimensional atom probe sample 200 is placed in the sample station 101 of the sample carrying module 1, the sample carrying module 1 is placed in the vacuum sealing tube 2, the vacuum sealing tube 2 is evacuated, and then the three-dimensional atom probe sample 200 is subjected to heat treatment. The vacuum sealing tube 2 is made of high temperature resistant material (such as quartz), and the vacuum sealing tube 2 can provide a vacuum environment for the three-dimensional atom probe sample 200 in the sample carrying module 1. Further, the temperature of the vacuum environment is controllable through an external heating system. The establishment of the vacuum environment effectively isolates the three-dimensional atom probe sample 200 from contacting with the external air, effectively prevents the sample from oxidation reaction, and provides a clean and stable heat treatment condition for the three-dimensional atom probe sample 200.
After the heat treatment is completed, the vacuum sealed tube 2 after the heat treatment is placed at a sealed tube station 302 of the cooling module 3, and the three-dimensional atom probe sample 200 is cooled by using cooling liquid. The cooling chamber 301 in the cooling module 3 may be filled with different types of cooling liquid, such as liquid nitrogen, liquid carbon dioxide or cryogenic ethanol, according to actual requirements, to achieve different cooling rates and final temperature control. The cooling liquid can be used for rapidly cooling and keeping the low temperature for a long time, so that the problem of component segregation or phase change caused by the room temperature standing effect is avoided. In the cooling process, the three-dimensional atom probe sample 200 is always in a vacuum sealing state, so that the sample is effectively prevented from oxidation reaction. After the cooling is completed, the three-dimensional atom probe sample 200 is taken out of the sample bearing module 1, and the three-dimensional atom probe sample 200 can be transferred to the three-dimensional atom probe equipment for characterization after being polished.
The processing device 100 for three-dimensional atom probe samples provided in the embodiments of the present disclosure provides a whole-course vacuum protection environment for the three-dimensional atom probe sample 200 through the vacuum sealing tube 2 in the processing process applied to the three-dimensional atom probe sample 200. Specifically, the three-dimensional atom probe sample 200 is placed in the vacuum-sealed tube 2 after rough polishing to avoid contact with air. The three-dimensional atom probe sample 200 then enters a thermal process flow to achieve precise temperature control by an external heating system. After the heat treatment is completed, the three-dimensional atom probe sample 200 is transferred to the cooling module 3 together with the vacuum sealing tube 2, and is rapidly cooled by using cooling liquid. Since the three-dimensional atom probe sample 200 remains in a vacuum environment throughout the cooling process, contact with air is further prevented. In the heat treatment and cooling stage, the three-dimensional atom probe sample 200 is always in a vacuum sealing state, so that the contact with the outside air is effectively isolated, and the three-dimensional atom probe sample 200 is prevented from undergoing oxidation reaction, thereby being beneficial to shortening the time of the preparation flow of the three-dimensional atom probe sample 200. In the cooling stage, the cooling liquid in the cooling module 3 can be used for rapidly cooling and keeping the low temperature for a long time, so that the problem of component segregation or phase change caused by the room temperature standing effect is avoided. Finally, after the temperature reduction is completed, the three-dimensional atom probe sample 200 is taken out of the vacuum sealing tube 2 and subjected to fine polishing treatment, and then is quickly transferred to the three-dimensional atom probe equipment for characterization. Through the vacuum and low-temperature protection mechanism of the whole flow, the accuracy of phase change analysis and component characterization of the subsequent materials is obviously improved, and the three-dimensional atomic probe data can truly reflect the microstructure characteristics of the three-dimensional atomic probe sample 200.
In some embodiments, the sample carrier module 1 is provided with a sample station 101. By providing multiple sample stations 101, multiple three-dimensional atom probe samples 200 can be processed simultaneously. The design improves the throughput and efficiency of the experiment, and is particularly suitable for the situation that batch analysis or comparison research is required.
In some embodiments, the sample station 101 is a mounting hole that mates with a fixed copper tube of the three-dimensional atom probe sample 200, where the fixed copper tube of the three-dimensional atom probe sample 200 can be inserted to effect fixation.
In some embodiments, the chamber 301 is provided with a plurality of sealed tube stations 302. The multiple sealed tube stations 302 allow for simultaneous processing of multiple vacuum sealed tubes 2 (one or more sample carrier modules 1 may be placed within each sealed tube), thereby significantly improving sample processing capabilities, which enables the experiment to complete more sample processing tasks in a shorter time.
In some embodiments, the seal tube station 302 is a mounting hole that mates with the vacuum seal tube 2, and the vacuum seal tube 2 may be inserted into the mounting hole to effect securement.
In some embodiments, the sample carrier module 1 comprises a sample carrier base 11 and a sample protective cover 12. The sample carrying base 11 is provided with a sample station 101. The sample protection cover 12 is detachably fastened to the sample carrying base 11, so as to place the sample station 101 inside. The sample carrying base 11 and the sample protecting cover 12 are designed to be connected in a detachable mode, so that after the three-dimensional atom probe sample 200 is placed on the sample station 101 of the sample carrying base 11, the sample protecting cover 12 is covered on the sample carrying base 11 to form a relatively closed space, and the damage to the three-dimensional atom probe sample 200 is avoided.
In some embodiments, the sample protection cover 12 is provided with a through hole 120. The through holes 120 provided in the sample protection cover 12 can supply heat to and from the space, which helps to regulate the heat exchange process of the three-dimensional atom probe sample 200 and helps to accurately complete the heat treatment process.
In some embodiments, the sample carrying base 11 and the sample protecting cover 12 may be detachably connected by means of a clamping connection. Or the sample carrying base 11 and the sample protecting cover 12 can be detachably connected in a threaded connection manner. Alternatively, the sample carrying base 11 is a cylindrical structure with threads on the outer peripheral surface, and one end surface of the sample carrying base 11 is provided with a sample station 101. The sample protection cover 12 has a cylindrical structure with threads on the inner peripheral surface, and is fastened to the sample carrying base 11 by screwing. By means of threaded connection, a repeatedly detachable fastening connection is formed between the sample carrying base 11 and the sample protecting cover 12. The user can complete the installation or separation of the sample carrying base 11 and the sample protecting cover 12 by rotating, so that the three-dimensional atom probe sample 200 can be conveniently loaded and taken out, and the equipment is convenient to clean and maintain.
In some embodiments, one end face of the sample carrying base 11 is provided with a plurality of sample stations 101. By providing multiple sample stations 101 in the sample carrier base 11, multiple three-dimensional atom probe samples 200 can be processed simultaneously. The design improves the throughput and efficiency of the experiment, and is particularly suitable for the situation that batch analysis or comparison research is required.
In some embodiments, the plurality of sample stations 101 are evenly distributed. The uniform distribution of sample stations 101 facilitates uniform conduction and distribution of heat across the load bearing base.
In some embodiments, the sample protection cover 12 includes a bottom plate 121 and a barrel 122, at least one of the bottom plate 121 and the barrel 122 being provided with a through hole 120. The inner circumferential surface of the cylinder 122 is provided with threads, and the bottom plate 121 is provided at one end of the cylinder 122, and the other end of the cylinder 122 is opened. Through holes 120 are formed in the bottom plate 121 and the barrel 122, so that the heat in-out path of the sample protection cover 12 and the sample bearing base 11 can be optimized, and the heat exchange process of the three-dimensional atom probe sample 200 can be regulated and controlled more accurately, so that the heat treatment process can be completed accurately.
In some embodiments, after the sample protection cover 12 and the sample carrying base 11 are snap-coupled, the distance between the bottom plate 121 of the sample protection cover 12 and the end surface of the sample carrying base 11 where the sample station 101 is located is between 10mm and 20 mm.
In some embodiments, the bottom plate 121 is provided with a plurality of through holes 120, and the plurality of through holes 120 are uniformly distributed. Taking the example that the bottom plate 121 is provided with 3 through holes 120, the 3 through holes 120 are uniformly distributed around the center of the bottom plate 121 at intervals. The bottom plate 121 is provided with through holes 120 having an aperture of between 0.5mm and 2mm, and adjacent through holes 120 have a pitch of between 3mm and 8 mm.
In some embodiments, the barrel 122 is provided with a plurality of through holes 120. Optionally, a plurality of through holes 120 are distributed along the circumference of the barrel 122. Optionally, a plurality of through holes 120 are distributed along the axial direction of the barrel 122. The cylinder 122 is provided with through holes 120 having an aperture of between 0.5mm and 2mm, and adjacent through holes 120 have a pitch of between 3mm and 8 mm.
In some embodiments, the plurality of through holes 120 of the barrel 122 are evenly distributed along the circumference of the barrel 122. Or the plurality of through holes 120 of the cylinder 122 are uniformly distributed along the axial direction of the cylinder 122.
In some embodiments, the cooling module 3 includes a cover 31, a housing 32, and a seal tube carrier 33. The housing 32 is provided with a chamber 301 for containing a cooling liquid, and has an opening. The cover 31 is detachably disposed at the opening of the housing 32. A seal tube carrier 33 is located inside the chamber 301 and is provided with a seal tube station 302. The housing 32 cooperates with the removable cover 31 to form a relatively airtight chamber 301. This not only facilitates convenient handling of the vacuum sealing tube 2 in the sealing tube station 302, but also avoids waste of the cooling liquid due to volatilization, so that the low temperature environment can be maintained in the chamber 301 for a long time.
In some embodiments, the outer wall of the housing 32 is a vacuum sandwich. The vacuum sandwich structure can reduce heat conduction and convection between the inside and the outside of the shell 32 in a vacuumizing manner, so that a better heat insulation effect is realized, and the chamber 301 can be maintained in a low-temperature environment for a long time.
In some embodiments, the outer wall of the housing 32 is provided with an insulating material (not shown). For example, the heat insulating material may be a composite structural layer which is composed of polyurethane material and ceramic fiber and has heat insulating function. By providing the heat insulating material on the outer wall, heat conduction and convection between the inside and outside of the housing 32 can be reduced, thereby realizing a preferable heat insulating effect, and being helpful for maintaining a low temperature environment in the chamber 301 for a long time.
In some embodiments, the outer wall of the housing 32 is a vacuum sandwich, and the sandwich is filled with a thermally insulating material. The vacuum interlayer reduces gas molecules by vacuumizing, so that heat conduction and convection can be remarkably eliminated, and the heat insulation material further blocks residual trace heat conduction and radiation heat transfer. The combination of the dual thermal insulation mechanism of the vacuum interlayer and the thermal insulation material greatly reduces the heat conduction and convection between the inside and outside of the housing 32, thereby realizing better thermal insulation and heat preservation effects and being beneficial to maintaining the low-temperature environment in the chamber 301 for a long time.
In some embodiments, the seal tube carrier 33 is provided with a plurality of seal tube stations 302. The multiple sealed tube stations 302 allow for simultaneous processing of multiple vacuum sealed tubes 2 (one or more sample carrier modules 1 may be placed within each sealed tube), thereby significantly improving sample processing capabilities, which enables the experiment to complete more sample processing tasks in a shorter time.
In some embodiments, the plurality of seal tube stations 302 are evenly distributed. The uniform distribution of the sealed tube stations 302 helps to create a more uniform temperature field throughout the chamber 301, subjecting all three-dimensional atom probe samples 200 to a similar cool down cooling process.
In some embodiments, the seal tube carrier 33 is a cylindrical structure, one end surface of the seal tube carrier 33 is connected to the bottom of the housing 32, and the other end surface of the seal tube carrier 33 is provided with a plurality of seal tube stations 302, and the plurality of seal tube stations 302 are uniformly distributed along the circumference of the seal tube carrier 33. The seal tube carrier 33 of cylindrical configuration is in contact with the coolant on both its inside and outside in the operating state, so that the seal tube station 302 provided thereon can receive cooling from multiple directions. This structure is advantageous in improving the uniformity of heat exchange of the vacuum sealing tube 2 during the cooling process, thereby improving the uniformity of cooling of the three-dimensional atom probe sample 200 inside thereof.
The vacuum sealed tube 2 is in a near vacuum environment, which inhibits heat conduction and heat convection in a gaseous medium, but also retains heat radiation and a heat exchange path realized by solid contact. Although the vacuum environment may relatively reduce the overall cooling rate of the three-dimensional atom probe sample 200, the lack of gas flow and local rapid heat dissipation effects helps to avoid uneven cooling due to temperature gradient differences, thereby improving the uniformity of the temperature distribution inside the three-dimensional atom probe sample 200. More importantly, the vacuum environment can effectively prevent the three-dimensional atom probe sample 200 from oxidizing and contaminating during heating or cooling.
In some embodiments, an air extraction valve (not shown) may be disposed on the cover 31 of the cooling module 3, and the air extraction valve may be used to adjust the air pressure in the chamber 301, so as to optimize the flow state and heat exchange efficiency of the cooling liquid, and further improve the cooling rate and the temperature control accuracy of the sample.
The embodiments of the present disclosure provide a processing method for a three-dimensional atom probe sample, and referring to fig. 8, the processing method is implemented based on the processing apparatus 100 for a three-dimensional atom probe sample provided in the foregoing embodiments, and the processing method includes:
s801, the three-dimensional atom probe sample 200 after rough polishing is placed at the sample station 101 of the sample carrying module 1.
In some embodiments, the three-dimensional atom probe sample 200 is first immersed in a rough polishing corrosive liquid for rough polishing, and after the rough polishing is completed, the three-dimensional atom probe sample 200 is placed in the sample station 101 of the sample carrying module 1.
In some embodiments, the three-dimensional atom probe sample 200 after rough polishing is placed at the sample station 101 of the sample carrying base 11, and then the sample protecting cover 12 is buckled to the sample carrying base 11 to form the complete sample carrying module 1.
S802, placing the sample bearing module 1 in the vacuum sealing tube 2, vacuumizing the vacuum sealing tube 2, and then performing heat treatment on the three-dimensional atom probe sample 200.
In some embodiments, during the heat treatment of the three-dimensional atom probe sample 200, the temperature of the heat treatment is not lower than 300 ℃, the duration of the heat treatment is not less than 10 minutes, and the vacuum degree in the vacuum sealing tube 2 is not higher than 1×10 -2 Pa. Alternatively, the heat treatment is performed at a temperature of 300 ℃ to 1200 ℃ for a period of 10min to 24h, and the vacuum degree in the vacuum sealing tube 2 is 1×10 -2 Pa to 1×10 -4 Pa.
S803, placing the vacuum sealed tube 2 after heat treatment at a sealed tube station 302 of a cooling module 3, and cooling the three-dimensional atom probe sample 200 by using cooling liquid.
In some embodiments, the temperature that can be reached by the cooling module 3 is between-196 ℃ and-50 ℃.
In some embodiments, the cooling rate of the temperature-reducing cooling process of the three-dimensional atom probe sample 200 is not less than 10 ℃ per second, and the temperature of the cooled three-dimensional atom probe sample 200 is not greater than-50 ℃. Alternatively, the cooling rate of the desuperheating cooling process of the three-dimensional atom probe sample 200 is 10 ℃ per second to 100 ℃ per second.
S804, after the temperature reduction is completed, the three-dimensional atom probe sample 200 is taken out from the sample carrying module 1.
In some embodiments, after the three-dimensional atom probe sample 200 is removed, the three-dimensional atom probe sample 200 may be polished and transferred to a three-dimensional atom probe device for characterization.
In some embodiments, when the temperature of the three-dimensional atom probe sample 200 is not higher than-50 ℃, the three-dimensional atom probe sample 200 is taken out from the sample carrying module 1, and the three-dimensional atom probe sample 200 is soaked in a polishing corrosive liquid for polishing. After finishing the finish polishing, the three-dimensional atom probe sample 200 is transferred to a three-dimensional atom probe device for characterization.
In some embodiments, the finish polishing time of the three-dimensional atom probe sample 200 should be controlled to be within 300 seconds. The time from the end of polishing of the three-dimensional atom probe sample 200 to transfer to the three-dimensional atom probe device should be controlled within 60 s.
In the embodiment of the present disclosure, the three-dimensional atom probe sample 200 is first roughly polished, and then the three-dimensional atom probe sample 200 is placed in the sample carrying module 1 and placed in the vacuum sealing tube 2. In the subsequent heat treatment stage and cooling stage, the three-dimensional atom probe sample 200 is not required to be taken out from the vacuum sealing tube 2, and the three-dimensional atom probe sample 200 is always in a vacuum sealing state, so that the contact between the three-dimensional atom probe sample 200 and the outside air is effectively isolated, the oxidation reaction of the sample is effectively prevented, and the time of the sample preparation process is shortened.
Taking the three-dimensional atom probe sample 200 as an example of an Al-Mg-Si alloy, immersing the three-dimensional atom probe sample 200 in a rough polishing corrosive liquid for rough polishing, after the rough polishing is completed, placing the three-dimensional atom probe sample 200 after the rough polishing in a sample station 101 of a sample bearing base 11, and then fastening a sample protection cover 12 on the sample bearing base 11 to form the complete sample bearing module 1. The rough polishing corrosive liquid is a solution formed by 10% perchloric acid and 90% glacial acetic acid, and the corrosion voltage in the rough polishing process is 8V.
Subsequently, the sample carrier module 1 is placed in the vacuum sealed tube 2, the vacuum sealed tube 2 is evacuated, and then the three-dimensional atom probe sample 200 is subjected to heat treatment. In the process of heat-treating the three-dimensional atom probe sample 200, the temperature of the heat treatment was 525 ℃, the duration of the heat treatment was 4 hours, and the degree of vacuum in the vacuum-sealed tube 2 was 5×10 -3 Pa.
Then, the vacuum sealed tube 2 after heat treatment is placed at a sealed tube station 302 of the cooling module 3, and the three-dimensional atom probe sample 200 is cooled by using cooling liquid. The temperature of the cooling liquid is-196 ℃, the cooling rate of the three-dimensional atom probe sample 200 is 80 ℃ per second, and the three-dimensional atom probe sample 200 is maintained for 30min under the condition that the temperature is not higher than-50 ℃.
After the three-dimensional atom probe sample 200 is cooled, the three-dimensional atom probe sample 200 is taken out from the sample carrying module 1, and the three-dimensional atom probe sample 200 is soaked in a polishing corrosive liquid for polishing. After finishing the finish polishing, the three-dimensional atom probe sample 200 was transferred to a three-dimensional atom probe device for characterization within 60 seconds. Here, the polishing etching solution is a solution formed by 4% of perchloric acid and 96% of ethylene glycol butyl ether, the etching voltage in the polishing process is 5V, and the polishing time is 250s.
The processing apparatus 100 and the processing method for a three-dimensional atom probe sample provided in the embodiments of the present disclosure may also be applied to other samples that need to undergo heat treatment and cooling, such as semiconductor material samples, ceramic material samples, optical material samples, and the like.
The above-described apparatus embodiments are merely illustrative, and for example, the division of the units may be merely a logical function division, and there may be additional divisions when actually implemented, for example, multiple units or components may be combined or integrated into another system, or some features may be omitted or not performed. In addition, the coupling or direct coupling or communication connection shown or discussed with each other may be through some interface, device or unit indirect coupling or communication connection, which may be in electrical, mechanical or other form. The units described as separate units may or may not be physically separate, and units shown as units may or may not be physical units, may be located in one place, or may be distributed on a plurality of network units. Some or all of the units may be selected according to actual needs to implement the present embodiment. In addition, each functional unit in the embodiments of the present disclosure may be integrated in one processing unit, or each unit may exist alone physically, or two or more units may be integrated in one unit.
Claims (16)
1. A processing apparatus for a three-dimensional atom probe sample, comprising:
the sample bearing module is provided with sample stations, and each sample station is used for placing a three-dimensional atom probe sample;
the vacuum sealing tube is used for accommodating the sample bearing module;
The cooling module is provided with a chamber for containing cooling liquid, and the chamber is provided with a sealing tube station used for placing a vacuum sealing tube.
2. The processing apparatus of claim 1, wherein the sample carrier module comprises:
the sample bearing base is provided with a sample station;
The sample protection cover is detachably covered on the sample bearing base to place the sample station inside.
3. The processing apparatus according to claim 1, wherein the sample protection cover is provided with a through hole.
4. The processing apparatus according to claim 2, wherein the sample carrying base has a cylindrical structure having a screw thread on an outer peripheral surface thereof, and one end surface of the sample carrying base is provided with a sample station;
The sample protection cover is of a cylindrical structure with threads on the inner peripheral surface, and is covered and buckled on the sample bearing base in a threaded connection mode.
5. A processing apparatus according to claim 3, wherein one end face of the sample carrying base is provided with a plurality of sample stations.
6. A processing apparatus according to claim 3, wherein the sample protection cover comprises:
a bottom plate;
The inner peripheral surface of the cylinder is provided with threads, the bottom plate is arranged at one end of the cylinder, and the other end of the cylinder is open;
At least one of the bottom plate and the cylinder is provided with a through hole.
7. The processing apparatus of claim 5, wherein the base plate is provided with a plurality of through holes.
8. A treatment device according to claim 5, wherein the cylinder is provided with a plurality of through holes distributed in the circumferential and/or axial direction of the cylinder.
9. The treatment device according to claim 8, wherein the plurality of through holes of the cylinder are distributed along the circumferential direction and/or the axial direction of the cylinder.
10. The processing apparatus according to any one of claims 1 to 9, wherein the cooling module comprises:
A housing provided with a chamber for accommodating a cooling liquid and having an opening;
the cover body is detachably arranged at the opening of the shell;
the sealing tube bearing seat is positioned in the cavity and is provided with a sealing tube station.
11. A treatment device according to claim 10, wherein the outer wall of the housing is of a vacuum sandwich construction and/or the outer wall of the housing is provided with a heat insulating material.
12. A handling device according to claim 10, wherein the seal tube carrier is provided with a plurality of seal tube stations.
13. The processing apparatus of claim 10, wherein the seal tube carrier is of a cylindrical configuration, one end face of the seal tube carrier is connected to the bottom of the housing, and the other end face of the seal tube carrier is provided with a plurality of seal tube stations.
14. A method of processing a three-dimensional atom probe sample, characterized in that it is realized based on a processing device for a three-dimensional atom probe sample as claimed in any one of claims 1 to 13, comprising:
placing the coarsely polished three-dimensional atom probe sample at a sample station of a sample bearing module;
Placing the sample bearing module in a vacuum sealing tube, vacuumizing the vacuum sealing tube, and then performing heat treatment on the three-dimensional atom probe sample;
Placing the vacuum sealing tube after heat treatment at a sealing tube station of a cooling module, and cooling the three-dimensional atom probe sample by using cooling liquid;
and after cooling is completed, taking out the three-dimensional atom probe sample from the sample bearing module.
15. The method of claim 14, wherein the parameter requirements of the thermal treatment process of the three-dimensional atom probe sample include at least one of:
The temperature of the heat treatment is not lower than 300 ℃;
The duration of the heat treatment is not less than 10min;
the vacuum degree in the vacuum sealing tube is not higher than 1×10 -2 Pa.
16. The method of claim 14, wherein the parametric requirements for the cool down process of the three-dimensional atom probe sample include at least one of:
the cooling rate is not lower than 10 ℃ per second;
the temperature of the three-dimensional atom probe sample after cooling is not higher than-50 ℃.
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